Textile-machinery lubricant composition

ABSTRACT

AN IMPROVED HIGH RETENTION LUBRICANT FOR TEXTILE-MACHINERY COMPRISES A NAPHTHENIC BASE OIL, A TACKINESS AGENT (E.G., POLYISOBUTYLENE), AND AN EFFECTIVE AMOUNT OF A LITHIUM SOAP (E.G. 0.1-1.5% LITHIUM STEARATE) TO PROVIDE A MECMICHAEL VISCOSITY AT 70* F. OF AT LEAST 15 (PREFERABLY 20-35). THE BASE OIL CAN HAVE A VISCOSITY IN THE RANGE OF 60-600 SUS AT 100* F. (MORE PREFERABLY 125300 SUS) AND AN ANILINE POINT IN THE RANGE OF 150-170* F., SAID BASE OIL COMPRISING AT LEAST ONE HYDROREFINED NAPHTHENIC OIL COMPONENT HAVING A VISCOSITY IN THE RANGE OF 40-12,000 SUS AT 100* F., AND PREFERABLY, IS A WIDE BOILING RANGE BLEND CONTAINING AT LEAST TWO SUCH HYDROREFINED NAPHTHENIC OILS. FOR EXAMPLE, THE LUBRICANT CAN COMPRISE 75 PARTS BY WEIGHT OF 100 SUS HYDROREFINED NAPHTHENIC OIL, 20 PARTS OF 2400 SUS HYDROREFINED NAPHTHENIC OIL, 2 PARTS OF A HIGH MOLECULAR WEIGHT (APPARENT M.W. IN OIL OF ABOUT 100,000) POLYISOBUTYLENE TACKINESS AGENT, 1 PART OF LITHIUM STEARATE, 1.5 PARTS OF CHLORINATED PARAFFIN AS AN ANTIWEAR AGENT, AND 5 P.P.M. OF SILICONE ANTIFOAM.

United States Patent U.S. Cl. 252--42.1 13 Claims ABSTRACT OF THEDISCLOSURE An improved high retention lubricant for textile-machinerycomprises a naphthenic base oil, a tackiness agent (e.g.,polyisobutylene), and an eifective amount of a lithium soap (e.g.0.l1.5% lithium stearate) to provide a MacMichael viscosity at 70 F. ofat least 15 (preferably 20-35). The base oil can have a viscosity in'the range of 60-600 SUS at 100 F. (more preferably 125- 300 SUS) and ananiline point in the range of ISO-170 F., said base oil comprising atleast one hydrorefined naphthenic oil component having a viscosity inthe range of 40-12,000 SUS at 100 F., and preferably, is a wide boilingrange blend containing at least two such hydrorefined naphthenic oils.For example, the lubricant can comprise 75 parts by weight of 100 SUShydrorefined naphthenic oil, 20 parts of 2400 SUS hydrorefinednapththenic oil, 2 parts of a high molecular weight (apparent M.W. inoil of about 100,000) polyisobutylene tackiness agent, 1 part of lithiumstearate, 1.5 parts of chlorinated paraffin as an anti-wear agent, andp.p.m. of silicone antifoam.

CROSS REFERENCE TO RELATED APPLICATIONS The present application is acontinuation-in-part of application Ser. No. 35,231, filed May 6, 1970;Ser. No. 60,642, filed Aug. 3,-1970 (now abandoned); Ser. No. 178,193,filed Sept. 7, 1971, and Ser. No. 178,479, filed Sept. 7, 1971.

The following patents and applications are related to the disclosure ofthe present application in that they disclose additives which are usefulin the present composition and/ or methods of obtaining hydrorefinednaphthenic oils (and other oils) which can be used to make the textilemachinery lubricant oil composition of the present invention.

The disclosure of all of the following applications and patents ishereby incorporated in the present application:

Serial 2 Filing Patent No. date No.

Issue date 730,999- 5-22-68 Pending A.U. 116

(COPA Appeal PA 9011) 3,813,338 Patented May 28, 1974 TABLE-ContinuedSerial Filing Patent Issue No date No. date Title 812,516. 2-19-69 3,619, 414 11-9-71 Catalytic Hydrofinishing of Petroleum Distillates inthe Lubricating Oil Boiling Range-Ivor W. Mills, Merritt C. Kirk, Jr.and Albert '1. Olenzak.

850,716. 8-18-69 Now abandoned.... Blended Hydrocarbon Oil and Processof ManufactureIvor W. Mills and Glenn R. Dimeler. Now abandoned.Hydrcrefined Lube Oil and Process of Manufacture- Ivor W. Mills andGlenn R. Dimeler. 4-4-72 Process for Preparing High ViscosityHydrorefined Cable Oil-Ivor W. Mills, Glenn R. Dimeler, William A.Atkinson and David A. Hofiman. Pending A.U. 116.-- Oil and Process ofManuiacture oi Blended Hydrorefined Oil-Ivor W. Mills and Glenn R.Dimeler.

3, 706, 653 12-19-72 Light-colored Highly Aromatic Oil and Process ofPreparation-Ivor W. Mills, Glenn R. Dimeler and Merritt C. Kirk, .Tr.

8-1-72 Hydroreflned Cable Oil and Process of Manufacture- Ivor W. Millsand Glenn R. Dimeler.

9-26-72 Hydraulic Oil CompositionJohn Q. Griffith, III, Edward S.Williams grid William H. Reiland,

Pending A.U. Hydraulic Oil Composition Containing a Blended BaseStock-John Q. Gn'flith, III, Edward S. Williams, William H. Reiland,Jr., Ivor W. Mills and Glenn R. Dimeler.

a High Viscosity Index Gary L. Driscoll, Irl N.

Duling and David S.

Olenzak.

Pending A.U. 117... Mist Lubricant Containing Polymeric Additive- JamesR. Amaroso, Walter J. Coppock, Thomas D. Newingham and Edward S.Williams.

Pending A.U. 117... Composition Comprising Stabilized Hydrocracked Lubeand an Antioxidant- Robert B. Bryer, William W. Grouse, Jr., John Q.Griflith, III, Thomas D. N ewingham and William H. Reiland, Jr.

Pending A.U. 165... Soap Thickened Hydraulic Oil Composition-John Q.Griffith, III, Edward S. Williams and William H. Reiland, Jr.

Pending A.U. 161-.. Hydrogenated Ethylene- Propylene CopolymerOils-Richard S. Stearns, Irl N. Duling and David S. Gates.

Pending A.U. 116..- Hydrorefined Lube Oil and Process of Manufacture-Ivor W. Mills and Glenn R. Dimeler.

Pending A.U. 116-.- Polyisobutylene Oil Having 1 Abandoned Aug. 12, 1972in favor of the present application.

BACKGROUND OF THE INVENTION A textile-machine lubricant must performsatisfactorily in textile-mill service where adequate lubricatingproperties must be combined with high retention (e.g., the ability tostay put in a bearing). Stray oil thrown from a bearing can find its wayto the cloth being manufactured and complicate the cleaning steps takenat the end of the process.

Prior art textile-machinery lubricants have been compounded with highviscosity index oils (e.g., solvent-refined paraffinic lube oil) and acombination of additives to give the necessary retention properties. Oneof these materials, a lithium soap, was finely dispersed in theparaffinic oil, but was not in complete solution. Under fieldconditions, the soap separated from the product. This problem of gelstability has been frequently mentioned in the prior art.

The present invention relates to an improved high retention lubricantfor textile-machinery which does not separate under field conditions,and which is equivalent or superior to prior art textile-machinery whichdoes not separate under field conditions, and which is equivalent orsuperior to prior art textile lubricants in such performancecharacteristics as lubricating, retention and cloth scourability andwhich does not discolor or degrade textile fibers.

This improved high retention lubricant is not only resistant toseparation but also has brighter appearance, produces less staining ifit comes into contact with fabric, and provides rubber seal protectionand conditioning. Furthermore, in mill trials this new lubricantprovided lower mill consumption of electrical power required by suchtextile-machinery as Draper Shuttleless Looms.

Among the relevant prior art are the following:

0.8. Pat. No. Patentee Glass/Sub a, et al. Stevens, et al Trent-mam, etal McCarthy, et al 8/58 Brunstrum, at. al 252 41 Donaldson, et al208/217 X Coppock 252/36 SUMMARY OF THE INVENTION An improved highretention lubricant for textile-machinery comprises a naphthenic baseoil, a tackiness agent (e.g., polyisobutylene, isotactic polypropylene,polyacrylates, etc.), and an effective amount of a lithium soap (e.g.,0.1-1.5 lithium stearate) to provide a MacMichael viscosity at 70 F. ofat least 15 (preferably 20-35). The base oil can have a viscosity in therange of 60-600 SUS at 100 F. (more preferably 125-300 SUS) and ananiline point in the range of 150-170 F., said base oil comprising atleast one hydrorefined naphthenic oil component having a viscosity inthe range of 40-12,000 SUS at 100 F., and preferably, is a wide boilingrange blend containing at least two such hydrorefined naphthenic oils.For example, the lubricant can comprise 75 parts by weight of 100 SUShydrorefined naphthenic oil, 20 parts of 2400 SUS hydrorefinednaphthenic oil, 2 parts of a high molecular weight (apparent M.W. in oilof about 100,000) polyisobutylene tackiness agent, 1 part of lithiumstearate, 1.5 parts of chlorinated paraflin as an antiwear agent, andp.p.m. of silicone antifoam.

The improved high retention lubricant for textilemachinery of thepresent invention comprises additives and a base oil having an SUSviscosity in the range of 60-600 at 100 F. (more preferably 125-300" R),consisting essentially of one or more hydrorefined naphthenic I oils ofthe lubricating oil viscosity range (e.g., 45-12,000

SUS at F.) and having an aniline point in the range of -190" F., morepreferred -170 F., a viscositygravity constant (VGC) in the range of0820-0899, more preferred 0840-0899, and an ultraviolet absorptivity(i.e. UVA) at 260 millimicrons, (i.e., 260 UVA) which is at least 40%less than that of an unhydrorefined naphthenic lube of the sameviscosity (VGC) and boiling range. Preferably, the UVA of the base oilat 335 millimicrons (i.e., 335 UVA) is in the range of 0.0 to 0.4(typically 002-02) and the ASTM D1500 initial color is less than 4.0(more preferably no greater than 2.5).

The additives comprise a tackiness agent and a lithium soap insufficient quantity to thicken the base oil and provide a minimumMacMichael viscosity, at 70 F., of 15 (more preferably in the range of20-35, typically about 25). The preferred tackiness agents are olefinpolymers (e.g., atactic polypropylene, or polyisobutylene rubber) andcan be partially or fully hydrogenated; however, any oil-compatibletackiness agent (e.-g., polyacrylates, Al oleate, or natural rubberobtained from dehydrated latex) can be used. The preferred range for thepolyisobutylene polymers as commercially available, as in dilution withoil (about 50%) is 0.3-6%, more preferably l-3%. In any event, theamount used must be sufiicient to cause the lubricant to be highlyretentive on a bearing; however, the amount must be less than that whichwill cause the lubricant to be stringy.

Another preferred additive is an antiwear agent which will not harmtextiles, most preferred is 03-10% of a chlorinated parafiin; however,0.22% of tricresyl phosphate or a combination of these two additives canalso be used. Optionally, the improved high retention lubricant fortextile machinery can also contain an antifoam (such as 05-20 p.p.m. ofactive silicone antifoam). Generally such antifoam is used as a dilutesolution or suspension containing about 1% of the active ingredient.

To further safeguard against discoloration, an antioxidant such as0.05-l% ditertiarybutyl paracresol (i.e., DBPC) can also be included.

In general, any additive used in the textile-machine lubricant of thepresent invention should have an acid number less than 25 and the total,compounded lubricant should have an acid number less than 0.5 and aneutral pH (preferably, 6.2-7.7, more preferred 6.8-7.2).

FURTHER DESCRIPTION The base oil can consist essentially of anarrow-boiling range, hydrorefined naphthenic lube of the desired SUSviscosity or the desired viscosity base oil can be obtained from a Widerboiling range blend of two or more narrowboiling range naphthenic oils(e.g., a 150 SUS base oil can be obtained directly by hydrogenation of aSUS distillate or can be obtained by hydrogenating a blend of 100 and2500 SUS distillate or, more preferred, the 150 SUS base oil can beobtained by blending a 100 SUS hydrorefined distillate with a 2500 SUShydrorefined distillate). Processes for obtaining such distillates andsuch hydrogenated oils are disclosed, for example, in the previouslyreferred to applications and patents of Mills and co-inventors. Suchoils are available under the trade name Sunthene.

Although the base oil can have a viscosity at 100 F. in the range of60-600 SUS, the preferred viscosity range is 125-30 SUS and, morepreferred, 140-220 SUS. When the viscosity of the base oil is less thanabout 125 SUS, the flash point becomes so low that it is difficult toheat the oil sufliciently to incorporate the lithium stearate. Generallythe oil should be heated to about 400 F. for proper lithium stearateincorporation.

A blended base stock can be advantageous in such additive incorporationsince the lithium can be first incorporated in a hot, higher flash pointcomponent oil (e.g., 2500 SUS) and the mixture cooled prior toincorporation of other additives and the lower flash point remainder ofthe base oil. This flash point problem was considerably less in makingprior art textile lubricants with parafiinic base oils since theparafiinic oils have generally much higher flash points for a givenviscosity at 100 F. than do hydrogenated naphthenic oils. Forlubrication of looms, and most other textile machinery, the viscosity ofthe base oil at 100 F. is preferably no greater than 300 SUS because ahigher viscosity base oil can produce a textile lubricant which causestoo great an increase in start-up torque of the machinery. However, aprotective coating for metals (e.g., firearms) can be made from the sameadditives as the textile machinery lubricant and in which the base oilhas a viscosity as high as 600 SUS at 100 F.

To improve such properties as color, flash point and oxidationstability, the base oil can also contain in the range of 05-15% ofhydrorefined paraffinic oil, solvent-refined parafiinic oil (see Ser.No. 178,193), naphthenic distillate, naphthenic-acid free naphthenicdistillate, polyolefin oils or hydrogenated polyolefin oils.

The base oils preferably contain less than 80 p.p.m. of basic nitrogen,more preferably less than 30 p.p.m. (in some cases (0-10 p.p.m.), andcan be those described in the previously cited applications of Mills eta1. and, more preferably, are blends of two or more hydrorefinednaphthenic oils (e.g., a 150 SUS blend of a 100 SUS at 100 F.hydrorefined naphthenic oil and a 2500 SUS at 100 F. hydrorefined oil)or a blend of hydrorefined naphthenic oil and hydrocracked paraffinicoil.

In the lubricant of the present invention, the base oil can have ananiline point in the range of 140-180, preferably the aniline point ofthe base oil is in the range of ISO-170 "F. to enable maintenance ofgood rubber seal condition. Preferably, the oil or blend of oils isselected so as to obtain a base with the desired viscosity, anultraviolet absorptivity at 335 millimicrons (i.e. 335 UVA) in the rangeof 001-04, more preferred 002-02, and an aniline point in the range of150-170" F. The hydrorefined naphthenic oil component of such a basestock will generally have an aniline point in the range of 140- 190,more preferred ISO-170 F.

Lubricants which are mostly paratfinic in structure have high anilinepoints and will shrink the rubber and make it hard. This permits thelubricant to leak. On the other hand, if the aniline points is below 150F., excessive swell often occurs and the seal may be cut and torn by therubbing surface, thereby allowing lubricant to bypass. Seal conditioningadditives can also be used to improve seal performance in the lubricant.

The phrases severe hydrorefining or hydrogenation refer to processesconducted in the presence of a hydrogenation catalyst at from about500-775" F., with hydrogen of 50-100% purity, and from 800-3000 p.s.i.of hydrogen at the reactor inlet (at total pressures from 800- 6000p.s.i.g.) at a fresh feed liquid hourly space velocity (LHSV) of from0.1-8.0 (usually below 2.0), preferably conducted either in vapor phaseor trickle phase. Such hydrogenation or severe hydrorefining is to bedistinguished from hydrocracking in that the production of overhead(i.e., hydrocarbons boiling below 485 F.) is less than 25% by volume perpass through the reactor (and, typically, less than Product recycle, forexample, as in US. Pat. 2,900,433, can be used to increase severity.Recycle liquid hourly space velocity can vary from 0 to 20; however, itis preferred to operate at total liquid throughputs that obtain atgreater than 25% of flooding velocity and more preferably at from 40-98%of flooding velocity.

Preferably, the temperature is below that at which substantial crackingoccurs, that is, no more than 20 weight percent (preferably less than10%) of the feed stock is converted to material boiling below 300 F. ina single pass through the reactor. Although the maximum hydrogenationtemperature which will not produce substantial cracking is somewhatdependent upon the space velocity, the type of catalyst and thepressure, generally it is below 750 F. but can be as high as 785 F. Toallow a margin of safety, it is preferred to operate below 700 F.(except when it is desired to obtain a hydrogenated oil containing moregel aromatics than are in the charge). At total pressures below about2000 p.s.i. the preferred temperature is below about 660 F., since abovethat temperature the degradation of oil viscosity can become large.

Typical of such severe hydrorefining methods, when conducted within theaforementioned processing conditions, are those of US. Pat. Nos.2,968,614; 3,993,855; 3,012,963; 3,114,701; 3,144,404; 3,278,420 and3,642 and those of the previously referred to copending applications,Ser. No. 622,398; 652,026; 636,493; 730,999 and 812,516. The termsseverely hydrorefined oil or hydrogenated oil include the products,within the lubricating oil boiling range, of such severe hydrorefiningor hydrogenation. One characteristic of a severely hydrorefined orhydrogenated oil is that the ratio of monocyclic aromatics to polycyclicaromatics is significantly greater than in hydrotreated oils orconventional distillate oils.

Where the desired hydrorefined oils is to be of the naphthenic class, apreferred charge to the hydrogenation reactor can be obtained by vacuumdistillation of naphthenic or mildly aromatic crude oils (as in US. Pat.No. 3,184,396), especially those crude oils wherein the 1500-3000 SUS(at F.) distillate fractions have viscosity-gravity constants from 0.84to 0.92. Preferably, such as charge stock should be substantially freeof naphthenic acids prior to the hydrorefining (thus, in some casesdistillation in the presence of caustic is advantageous). Usuallymaterials boiling below about 600 F. (including residual H S, NH etc.)are removed from the hydrorefined oils, as by atmospheric distillation(and the viscosity can also be adjusted by choice of distillation endpoint) prior to clay contacting (if the oils are to be clay finished).Such naphthenic distillate oils are available commercially under thetrade name Circosol.

The viscosity of the base oil, or of the final hydrorefined oil, can beadjusted by the addition of other oils of higher or lower viscosity andwhich are within the lube oil boiling range. Where desired, the basicnitrogen content can be lowered by contacting the charge or hydrogenatedoil or the blend of hydrogenated oils with suflicient acidic adsorbentor mineral acid to reduce the basic nitrogen content of the oil, as tobelow 10 p.p.m.

By naphthenic distillate, we refer to a distillate fraction (or a mildlyacid treated distillate fraction, or a solvent rafiinate fraction or anacid-treated rafiinate) usually from vacuum distillation, or a crudewhich is classified as naphthenic (including relatively naphthenic) bythe viscosity-gravity constant (VGC) classification method. (See p.79-80 Plasticizer Technology, vol. 1, p. 5, Bruins, Reinhold PublishingCorp., N.Y., 1965.) Preferably, such crudes are Grade A (wax-free),typically Gulf Coastal, and include, for example, Refugio, Mirando, andBlack Bayou. The lower VGC oils can be obtained from midcontinentalcrudes; and can be dewaxed if desired (as by extraction orisomerization). Such naphthenic fractions will have a VGC in the rangeof 0.820 to 0.899 and, typically, a viscosity in the range of ISO-12,000SUS at 100 F. (for example, 500-6000). In some cases the crude (anddistillate) can have a VGC as high as 0.94 (such crudes arecharacterized as mildly aromatic), or higher (e.g., 096+). Deep furfuralextraction (e.g., about 50% yield) of a high VGC Grade A crude can beused to produce a wax-free, lower VGC fraction (e.g., 0.83 VGC).

Typically, paraffinic oils are those having a viscositygravity constant(VGC) in the range of 0.790 to 0.819 (preferably above 0.799). Typicalof solvent refined paraffinic lubes are those available commerciallyunder the trade name Sunpar. Typical hydrorefined paraflinic lubes arethose available commercially under the trade name Sunpar, H series(e.g., Sunpar' llOH).

Naphthenic oils have a VGC in the range of 0.820 to 0.899 and thepreferred hydrorefined naphthenic oils have a VGC in the range of 0.850to 0.899. Hydrorefined, relatively aromatic oils, having a VGC in therange of 0.900 to 0.920, can sometimes be used as a whole or partialsubstitute for the hydrorefined naphthenic lube. Aromatic oils(including hydrorefined or hydroaromatized oils) having a VGC in therange of 0.921 to 1.050 and greater, canbe useful in minor proportions(e.g., 1-20%) for adjusting the aniline point of the base oil,particularly when the base oil contains a high proportion (e.g., 20%) ofa high VI hydrocracked paraflinic oil.

As an additional component to the hydrorefined naphthenic oilspreviously described, the lubricant can contain a hydrogenatedpolyolefin oil (e.g., see Ser. No. 220,362 of Stearns et al.; Ser. No.52,301 of Driscoll et al.; Canadian Pat. 842,290; and U5. Pat.3,598,740) or a high viscosity index, hydrocracked oil or a mixture ofsuch components. (Such oils can be dewaxed, if desired). In such blendsan aromatic oil or concentrate rich in aromatic hydrocarbons (e.g.,cycle oil) may have to be added to obtain the proper aniline point forseal swelling.

The preferred polyolefin oils are polymers or copolymers of C -C olefinwhich have a pour point no greater than --35 F., and preferably below 50F. The hydrogenation can be from 50% to 100% of saturation and,preferably, is to a bromine number no greater than 10, more preferablyless than 5, Preferred polyolefins include ethylene-propylene copolymer,polypropylene, polybutene (especially polyisobutylene), andpoly(1-octene).

The high VI hydrocracked parafiinic oil component can be obtained byhydrocraclring a high viscosity distillate or dewaxed distillate from aparafiinic crude (such as Lagomedio) and typically has a VI in the rangeof 90-105 and contains in the range of 330% of aromatics by clay-gelanalysis. The hydrocracked lubes are preferably stabilized (against UVlight degradation and sludging) by extraction of the hydrocracked oilwith aromatic selective solvents, such as furfural or phenol or byhydrorefining to reduce the 260 UVA at least 30% (preferably 40% Forexamples of such oils see Ser. No. 178,193 of Bryer et al.

' and US. Pat. 3,579,435 to Olenzak et al.

The preferred stabilized hydrocracked oils (whether extracted orhydrorefined) are characterized by having a D-943 test life (to anincrease in acid number of 2.0) which is at least 20% lower than theD-943 life of an unstabilized hydrocracked oil but which is at least 20%greater than the D-943 life (with the usual amount of inhibitor, e.g.,0.5% DBPC) of an unhydrocracked solvent refined parafiinic lube of thesame viscosity.

The preferred soap is lithium stearate; however, any of the prior artlithium soaps which have been used in petroleum lubricants can be usefulin textile oils of the present invention. Such soaps are shown, forexample, in U.S. Pats. 2,489,300 and 3,383,312. For soap thickening, thepreferred lithium soaps include soaps of fatty acids containing in therange of 12-22 carbon atoms, preferably an unsubstituted fatty acid.Stearates, palmitates, tallates, laurates, oleates and mixed soaps areamong the useful soaps.

ILLUSTRATIVE EXAMPLES In the following examples, as elsewhere in thisapplication, UVA stands for ultraviolet absorptivity, all percentagesare by weight and all viscosities are at 100 F., unless otherwise noted.

Example I A high retention, textile machinery lubricant was com poundedusing a base oil comprising hydrogenated naphthenic oil, and containinghigh molecular weight polyisobutylene (as a tackiness agent) and lithiumstearate.

The textile machinery lubricant composition had a MacMichael viscosityof about 25 at 70 F. and contained at 150 SUS (at 100 F.) base Oilhaving an aniline 8 point of 1 62 and consisting of 19.30 parts of 2400SUS (at 100 F.) hydrorefined naphthenic oil containing 45% aromatics andhaving a 260 UVA of 5.7 and a 335 UVA of 0.22 and 76.38 parts of 100 SUS(at 100 F.) hydrorefined naphthenic oil containing 35% aromatics andhaving a 260 UVA of 2.3 and a 335 UVA of 0.03. Both hy-j drorefinednaphthenic oils were obtained from naphthenic acid-free, naphthenicdistillate by hydrogenation at 625 F., 1200 p.s.i.g. of hydrogen, 0.2LHSV with a presulfided Ni-Mo-oxide catalyst. Before hydrorelining theSUS distillate had a 260 UVA of 7.3, a 335 UVA of 0.23 and contained 44%aromatics; whereas, the 2500 SUS distillate had a 260 UVA of 10.5, and335 UVA of 0.68 and contained 47% aromatics.

In addition to the base oil, the textile-machinery oil contained 1.9parts of commercial polyisobutylene (available under the trade namePartac-N of Enjay Company), 0.7 parts Li stearate, 0.4 parts of DBPCantioxidant, 0.02 parts of a defoamer containing 1% active ingredients(Dow Corning Silicone), and 1.3 parts of chlorinated paraffin (Chlorafin40), containing 40% chlorine. The chlorinated parafiin impartsespecially useful antiwear properties and does not discolor or damagetextiles. The degree of chlorination of this additive can varyconsiderably, depending on the manufacturer and grade; however, all suchpresently commercially available light colored, chlorinated paraffinscan be used in the lubricant of the present invention.

The compounding procedure follows:

Compounding procedure:

1. Mix all of the Li-stearate with all of the 2500 SUS oil and heat to400-410 F. for 10 minutes with mechanical agitation.

2. Stop heat and add 100 SUS oil-cool as quickly as possible, to about150 F.

3. Add remaining additives at l40-150 F.

4. Continue agitation until blend cools to 130 F.

Example 2 A textile-machinery lubricant was compounded using the sameadditives and procedures as that of Example 1, except that the base oilwas a 150 SUS solvent refined parafiinc lube (sold as Sunpar having aVGC .of 0.803, viscosity at 210 F. of about 43.6 SUS and an anilinepoint of 221. The paraflinic lube was made by blending two commerciallyavailable solvent refined paratiinic distillates, Sunpar 110 (75.55parts) and Sunpar (20.00 parts).

Example 3 Another lab evaluation was conducted in a complete Alemitelubrication system. In this study the lubricator was pulsed on 3-minutecycles or about 16 times faster than normal in plant operation. Eachlubricant was run for 700 hours, which would be equivalent to about11,000 hours in the field. Moreover, during the test, the lubricatorstand was constantly vibrated by a small eccentric electric motor topromote the separation and/or stratification of the oils.

The results confirmed those from the centrifuge test of Example 3. Theoil of Example 1 showed no tendency to separate or stratify under theseconditions. In addition,

the critical system components, including the filter and Example TheExample 1 oil also had other required textilemachine oil properties. TheExample 1 oil was subjected to a special test to measure the retentionor anti-leak charatcteristics of machine oils. The test correlates withthe field performance, and for this reason was used to compare theExample 1 oil with the Example 2 oil and with a conventional machine oilwhich contained no additives to improve oil retention.

The special test apparatus was a combination of iron nipples, unionsleeves, and elbows. They were joined together hand tight in a U-shapeand spot-welded to hold a fixed position. In the test 300 ml. of oilwere poured into the apparatus and it was then pressurized to 30 p.s.i.with nitrogen and allowed to stand at the selected test temperature forone hour. The oil that leaked from the apparatus was collected andweighed.

There was no significant difference in leakage between the Example 1 andExample 2 oil, both giving about times less leakage than theconventional oil.

However, the Example 1 oil has a leak-reducing feature not found in theExample 2 oil. The Example 1 oil keeps rubber seals soft and pliable andcauses them to swell slightly, thus, eliminating afield usage problem ofseal shrinkage. The difference between the Example 1 and Example 2 oilsis demonstrated by the following lab 'data:

Rubber Swell Test, percent, 212 -F., 168 hrs.

Example 1 oil +8.2 Example 2 oil -0.1

Buna N seals swell in the Example 1 oil and, thus, keep snug tolerancesand prevent leakage which takes place in usage due to wear.

Thus, the Example 1 lubricant has a combination of good retentionproperties plus the seal-conditioning feature which results in lessstray oil in textile plants than with the Example 2 lubricant.

Example 6 Even with the excellent retention properties of the Example 1lubricant, in field usage it will occasionally come into contact withcloth. It is important, therefore, that the oil not weaken the fabricafter the finishing steps are completed.

The damaging potential of textile machine oils can be evaluated by themethod of the Institute of Textile Technogoly (I'IT). In the evaluation,the test oil is run for eight hours in a laboratory-mounted bearing tosimulate used lubricant conditions. During this period, the bearingtemperature is recorded (it was essentially the same for the lubricantof Example 1 and the lubricant of Example 2, running between 105 and 110F.).

When the sample preparation is' complete;'the'oil is" applied to desizedcotton test fabric. Before bleaching,

one-half of the contaminated fabric samples, as well ascontrol pieces,are treated with 1% sulfuric acid solution for 30 minutes. The testpieces are then boiled one hour in 2% caustic, rinsed with tap water,bleached with a hydrogen peroxide solution for one hour, rinsed anddried. The samples and controls are then subjected to a "armpit-LLllQILQQI. 2

Fabric break strength, percentof control sample:

With acid treatment, 97. 6 94. 8 Without acid treatment 87.8 89. 1

These data show that both are excellent in terms of cloth scourabilitywith minimum fiber damage.

The Example 1 oil also produced less staining of cloth. These testresults caused the Example 1 oil to obtain the highest possible I'ITrating and make it applicable in all textile plants.

Example 7 Commercial lubricants Example 1 Description B C D lubricant lLoom test:

Gear temperature, F.

Motor side +17 +44 +30 +17 Other side +45 +36 +17 Power costs, percen+5. 5 +7. 9 5. 7 Overall performance. Unsatisfactory SatisfactoryAverage of two tests. 3 Data relative to Example 2 oil.

The Example 1 lubricant was the only oil which provided power savings.The temperature differences were not considered significant. Oil B wasGulf Harmony 121, Oil C was Texaco Rock Drill 1543' and Oil D was HumbleNuto 113.

In a test at another southern mill, the lubricating properties of theExample 1 lube were found to equal those of the Example 2 oil, but theExample 1 oil had better staining and removal properties. No separationproblems were note The examples above show that the Example 1 lubricantnot only solves the separation problem noted occasionally in the fieldwith prior art oils, but it also has lighter color and brighterappearance and causes less staining should it come in contact withfabric during manufacture.

In addition to the stability. and appearance, the Example 1 lubricantconditions and protects rubber seals and provides lower mill powerconsumption and cost. The Example 1 oil is also useful as a militaryautomotive and artillery grease. The preferred range (ISO- F.) ofaniline point. for the base oil disclosed herein is not necessarily thepreferred range if non-hydrocarbon seal swelling agents are contained inthe lubricant. For other rubbers than buna-N, neoprene, -etc., suchasthe silicones a diiferent aniline point range may be required forproper swellin (e.g.,- -for silicone rubbers an; aniline point in the arange 0f-195-2 15. F. is preferred).

'Thefollowing" Table lflists the properties of the textile'-" machinerylubricant of Example l, which is a lubricant of the present invention.The table also lists a preferred range for these properties; however,the lubricant of the present invention'need not have properties withinthisrange.

Tables 2 and 3list typical properties of commercially availablenaphthenic'lubes (before and after hydrorefining) which can be used inpractice of the present invention. The distillate oils are sold underthe trade name Circosol and the hydrorefinedoils are sold under thetrade name Sunthene.

TABLE 1 Preferred range Property Method 1 Example 1 of propertiesViscosity, MacMichaei/70" F--. 25 20-35. Flue ,CO F D92 280 270min.Fire, COG, F- D 330. 310 min.

our, F D97 20 Color D1600 2.5. 3.5 max. AP arnnm Visual Slight haze pCopper strip, class, 212 F., 3 hr Sulfur, percent- Conradson carbon,percent- Aniline point, F

Ash, nnronnt Suliated ash- Foam, tendencyfstability Sequence 1, ml-Sequence 11, ml Sequence 111, ml.

Busting, distilled wa 50/0 max. 50/0 max. Pass.

4-ball wear scar: 25 kg., 1,800 Lithium, p D m Chlorine, percent l ASTMtest method numbers.

1 Calculated from data obtained by picnometer. Accurate results cannotbe obtained using a hydrometer.

TABLE 2.TYPICAL DATA, COMMERCIALLY AVAILABLE HYDROREFINED NAPHTHENICLUBES Property ASTM test 011 1 Oil 2 Oil 3 Oil 4 Oil 5 Oil 6 Oil 7 Oil 8Viscosity, SUS at 100 F D2l6166 104 155 210 502 780 1, 275 2, 206 5,0Viscosity, SUS at 210 F D2l6166 38. 41. 0 43. 1 52. 0 59. 0 67. 7 84. 7126. API Gravity at 60 F 13-287-67 24. 2 23. 3 22. 5 20. 6 19. 9 19. 318. 6 19. 0 S 1110 gravity at 60 F D-1250-56 9088 9140 9190 9303 93509380 9427 9402 ash point, 000, F D-92 66 330 335 345 385 365 400 440 470Volatility, 22 hours at 225 F. wt. percent D 972-56 6. 38 5. 4. 57 2. 531.81 1. 00 0.23 0. 02 Pour point F D-97-06 30 -25 -1O -5 0 +15 +20color, 151 11 13-1500 13-15110-64 0.5 0.5 0.5 1.0 1.0 1.0 1.5 1.5 U.V.absorptivity at 260 mu D-2008-68 2. 2 3. 0 3. 4 4. 1 4. 8 5. 3 5. 7 6.7M hammwnivht '.D250267 205 325 330 355 370 380 400 450 Viscosity-gravityconstant D-2501-67 .871 .873 .875 878 .881 .881 .882 .871 Refractiveindex, n D-1747-62 1.4986 1.5015 1.5039 1.5104 1. 5130 1. 5146 1.5170 1. 5174 Reflectivity intercept D-2159-64 1.0460 1. 0463 1. 0463 1.0471 1. 0473 1. 0474 1. 0475 1. 0491 Carbon type analysis:

Aromatic carbon atoms, C... percent 15 16 16 15 17 18 18 1s Naphtheniccarbon atoms, (30, Percent D-2i40-62 42 42 42 43 41 41 41 36 Paraflmiccarbon atoms, Cg, percent 43 42 42 42 41 41 41 46 Molecular typeanalysis (clay gel):

Asphaltenes, wt. percent 0 0 0 0 0 0 0 0 Polar compounds, Wt. percent 0.2 0. 4 0. 5 0. 7 0.8 1.0 1. 1 2. 0

Aromatics, wt. percent..- D-2007- 34. 8 37. 6 38.5 42. 3 43. 2 43. 0 43.9 41. 8

Total aromatics, wt. per 35. 0 38. 0 39. 0 43.0 44. 0 44.0 46. 0 43. 8

saturates, wt. percent 65. 0 62. 0 61. 0 57. 0 56.0 56. 0 55. 0 56. 2Aniline point, F D611-64 156 160 162 164 171 174. 0 176. 0 193 ASTM typeD-2226-69 103 103 103 103 103 103 103 103 Norm-Oils 2, 3, 5 and B areblends oi oils 1 and 7.

TABLE 3.-TYPICAL DATA, COMMERCIALLY AVAILABLE NAPHTHENIC DISTILLATE OILSASTM ASTM Property designation 011 A Oil N o. 3 011 B 011 0 011 D Oil E011 F 011 G 011 H Viscosity, sus at F D-2161-c6 108 156 208 310 515 7301,276 2, 525 5,945 Viscosity, SUS at 210 F- Ill-2161 60 38. 2 41 43.246. 8 52. 4 58. 8 68 87. 2 135 API gravityo! 60 F"--- D-287-67 22. 2 22.4 21. 0 20. 1 19. 6 19. 1 18. 4 17. 6 17. 3 Specific gravity at 60 FD-1250-56 9206 9194 .9279 9334 9365 9396 9440 9490 9509 F ash 101111,000, F D-92-66 e20 330 345 355 380 330 495 Volati ty 22 hrs. at 225 F.,wt. percent"--- D-972-50 7. 58 5. 96 5. 40 4.35 3. 08 2. 11 l. 67 0.160.02 Pour point F 9766 -15 35 -30 -15 -10 -5 0 +10 +20 0010 101 1113-1500 134500-34 1. 25 1. 75 1.15 2.0 2.0 2.5 3.0 3.5 5. 75 M l ular wight D-2502-67 295 325 325 345 355 370 380 395 450 Viscosity-gravityconstant D- 501-6 0.884 0.878 0.884 0.887 0.885 0. 885 0. 885 0.889 0.884 Relractive index D-1747-62 1- 5031 l- 5079 1. 5121 1. 5160 1.5167 1. 5190 1. 5210 1. 5222 1. 5250 Beiractivity intercept13-2159-64 1. 0502 1. 0479 1. 0500 1. 0511 1. 0503 1. 0510 1. 0508 1.0495 1. 0495 Carbon type analysis:

Aromatic carbon atoms, 0. percent 21 20 21 22 21 22 22 21 2o Naphtheniccarbon atoms, C percent- D-2140-62 37 36 37 36 37 30 36 39 38 Paraflniccarbon atoms, 0.. percent 42 44 42 42 42 42 46 4o 42 Molecular typeanalysis (clay gel):

As haltenes, wt. percent-....'. 0 0 0 O 0 0 0 0 0 Po Compounds, wt.percent. 1. 1 1. 2 1. 8 2.0 2. 5 2. 7 8. 0 2. 7 4. 2

Aromatics, wt. percent.. D-2007-56'l 43. 0 41. 7 44. 0 44. 0 43. 8 43. 644. 0 44. 8 44. 7

Total aromatics, percent 44. 1 42. 9 45. 8 46. 0 46. 3 46. 3 47. 0 47. 548. 9

saturates, wt. percent 55.9 57. 1 54. 2 54. 0 53. 7 53.7 53. 0 52. 5 51.1 Aniline point, F D-611-04 156 152 154 156 162 166 172 183 ASTM type13-2226-09 103 103 103 103 103 103 103 103 103 Norm-Oils B, C, E and Fare blends 0! oils A and G.

' the range of 40-12,000 SUS at 100 F said tackiness agent polymer, andnatural rubber obtained from dehydrated.

0.01-0.4 and an aniline point in the range of ISO- F.,

and containing in the range of 85-100% of at least one hybeing selectedfrom the group consisting of polyacrylates, aluminum oleate, olefinpolymer, hydrogenated olefin polymer, mixtures of hydrogenated andunhydrogenated olefin latex.

2. A lubricant according to claim 1 wherein said base oil contains awide boiling range blend of at least two bydrorefined naphthenic oilcomponent having a viscosity in 75 drorefined naphthenic oils.

3. A lubricant according to claim 1 and having a Mac- Michael viscosityin the range of 20-35 and wherein said base oil has a viscosity at 100F. in the range of 125- 300 SUS.

4. A lubricant according to claim 3 wherein said tackiness agent ispolyisobutylene or hydrogenated polyisobutylene or a mixture ofpolyisobutylene and hydrogenated polyisobutylene.

5. A lubricant according to claim 4 and containing 0.1- 1.5% lithiumstearate.

6. A lubricant according to claim 5 and containing 03-10% of achlorinated parafiin or 0.22% of tricresyl phosphate, as an antiwearagent.

7. A lubricant according to claim 6 and containing 0.5- 20 p.p.m. of asilicone antifoam.

8. A lubricant according to claim 7 and containing 0.05-1% ofditertiarybutyl paracresol as an antioxidant.

9. A lubricant according to claim 1 wherein said base oil contains inthe range of 05-15% of hydrorefined paraffinic oil, solvent-refinedparafiinic oil, naphthenic distil- 20 late or naphthenic-acid freenaphthenic distillate.

10. A lubricant according to claim 1 where the aniline point of saidhydrorefined naphthenic oil component is in the range of ISO-170 F.

11. Hydraulic oil according to claim 1 wherein said lithium soap is asoap of a C -C fatty acid.

ness agent is selected from the group consisting of polyacrylates,hydrogenated olefin polymer, mixtures of hydrogenated and unhydrogenatedolefin polymer and natural rubber obtained from dehydrated latex.

References Cited UNITED STATES PATENTS Mikeska et a1. 25249.8 X Prutton252-42.1 X Morgan 252-36 Bax et al 252---36 Coshburn 25236 X Griifith eta1 2524'1 X PATRICK P. GARVIN, Primary Examiner A. H. METZ, AssistantExaminer U.S. Cl. X.R.

